粉状白钨酸的研究(Ⅴ)——12-钨磷酸的直接制备以及用正丁醚的提纯法

高等学校化学学报 ›› 1985, Vol. 6 ›› Issue (8): 674.

粉状白钨酸的研究(Ⅴ)——12-钨磷酸的直接制备以及用正丁醚的提纯法

顾翼东, 崔美芳

复旦大学化学系

收稿日期:1984-03-16 出版日期:1985-08-24 发布日期:1985-08-24

Studies on White Powdery Tungstic Acid (Ⅴ)——Direct Preparation of 12-Tungstophosphoric Acid from White Powdery Tungstic Acid and Its Purification through n-Butyl Ether Extraction

Gu Yidong, Cui MeiFang

Department of Chemistry, Fudan University, Shanghai

Received:1984-03-16 Online:1985-08-24 Published:1985-08-24

摘要/Abstract

摘要： 12-钨磷酸的应用,近年来发展迅速,有从实验室合成转为工业生产的趋势。本报告从E.Drechsel法的以钨酸钠和磷酸氢二钠为原料,改为以活性粉状白钨酸为原料,与磷酸直接反应,即成12-钨磷酸溶液。这样便可以免除Drechscl乙醚萃取法中大量盐酸的使用。在提纯时,把在Drechsel方法中所用的乙醚,改为沸点高的正丁醚,配合适当少量的盐酸,可以得到相应的(钅羊)盐油状物。并由于该(钅羊)盐安定度较差,用水反萃取即可使12-钨磷酸转入水溶液,经过浓缩即可得到12-钨磷酸晶体。回收的正丁醚,毋需蒸馏,可以反复使用。

Abstract: The white powdery tungstic acid prepared according to previous reports^[1,2] reacts directly with phosphoric acid solution to form a solution of 12-tungstophos-phoric acid with some other polytungstates.For purification, the solution was extracted with n-butyl ether under suitable addition of hydrochloric acid, so as to produce an oily layer which is not miscible with water and excessive n-butyl ether. The n-butyl ether layer was then stripped with water to obtain pure aqueous solution of 12-tungstophosphoric acid. On evaporation by heating, 12-tungstophosphoric acid gradually separated out as pure crystals.

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顾翼东, 崔美芳. 粉状白钨酸的研究(Ⅴ)——12-钨磷酸的直接制备以及用正丁醚的提纯法. 高等学校化学学报, 1985, 6(8): 674.

Gu Yidong, Cui MeiFang. Studies on White Powdery Tungstic Acid (Ⅴ)——Direct Preparation of 12-Tungstophosphoric Acid from White Powdery Tungstic Acid and Its Purification through n-Butyl Ether Extraction. Chem. J. Chinese Universities, 1985, 6(8): 674.